CN104949895A - Analysis method for determining recovery coefficient of shale pyrolysis parameter - Google Patents
Analysis method for determining recovery coefficient of shale pyrolysis parameter Download PDFInfo
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Abstract
The invention provides an analysis method for determining a recovery coefficient of a shale pyrolysis parameter. The analysis method comprises the following steps: step 1, grinding a shale sample, and adding liquid nitrogen at the same time; step 2, weighing the ground sample, putting the sample into a crucible special for a pyrolysis instrument, and putting the special crucible into the liquid nitrogen; step 3, taking out the special crucible from the liquid nitrogen, putting the crucible to the crucible position for pyrolysis analysis by the pyrolysis instrument; and step 4, carrying out pyrolysis analysis on the same sample at normal temperature to obtain the hydrocarbon content lost in conventional pyrolysis analysis so as to calculate the recovery coefficient. According to the analysis method for determining the recovery coefficient of the shale pyrolysis parameter, loss of natural gas and light dydrocarbon in the sample is reduced; and compared with conventional pyrolysis analysis, the analysis method disclosed by the invention has the advantages that the recovery coefficient of the shale pyrolysis parameter is obtained.
Description
Technical field
The present invention relates to In Oil Field Exploration And Development technical field, particularly relate to a kind of analytical approach determining shale pyrolysis Parameter reconstruction coefficient.
Background technology
In common shale samples analytic process, due to reasons such as volatilizations, gaseous hydrocarbon (C
1-C
7) component can lose very soon.In addition, S
1can only detecting portion higher than C
30free hydro carbons.Therefore conventional pyrolysis S
1peak to be generally less than in shale contained can extractable organic matter (EOM), need to correct.In general, pyrolysis peak S
1in NF part heavy hydrocarbon, non-hydrocarbon and asphaltene, generally appear at pyrolysis S
2in peak, although composition pyrolysis S
2the hydro carbons majority at peak is derived from kerogen cracking, but also comprises some heavy hydrocarbons, the pyrolysis of non-hydrocarbon and asphaltene and thermal evaporation.
Therefore, when evaluating shale oil-containing tolerance by pyrolysis parameters of rock, be necessary to carry out pyrolysis S
1lighter hydrocarbons recover and pyrolysis S
2in determination two research of solvable hydrocarbon content, and pyrolysis S
1lighter hydrocarbons correction coefficient and pyrolysis S
2heavy hydrocarbon scale-up factor is referential pyrolysis analysis method not.We have invented a kind of analytical approach of new determination shale pyrolysis Parameter reconstruction coefficient for this reason, solve above technical matters.
Summary of the invention
The object of this invention is to provide a kind of analytical approach determining shale pyrolysis Parameter reconstruction coefficient when evaluating shale oil-containing tolerance.
Object of the present invention realizes by following technical measures: the analytical approach determining shale pyrolysis Parameter reconstruction coefficient, and this determines that the analytical approach of shale pyrolysis Parameter reconstruction coefficient comprises: step 1, is ground by core sample, and grinding limit, limit adds liquid nitrogen; Step 2, takes the sample after grinding, puts into pyrolysis instrument special copple, and special copple is put into liquid nitrogen; Step 3, takes out special copple and puts into crucible position and adopt pyrolysis instrument to carry out pyrolysis analysis from liquid nitrogen; And step 4, identical sample being carried out pyrolysis analysis after normal temperature is placed, obtaining the hydrocarbon content of conventional pyrolysis analysis loss, for calculating coefficient of restitution.
Object of the present invention also realizes by following technical measures:
This determines that the analytical approach of shale pyrolysis Parameter reconstruction coefficient also comprises, and before step 1, chooses new core-drilling sample sealing freezen protective; And open pyrolysis instrument stabilizer instrument.
In the step opening pyrolysis instrument stabilizer instrument, open the ventilation of pyrolysis instrument and stablize 2 hours, then carry out school machine, keep holding state.
In step 1, liquid nitrogen is poured in copper mortar, and by pyrolysis instrument special copple, hammer, these instrument freezing processing of tweezers, keep it at low-temperature condition, the mortar of cooling processing put into by the inner uncontaminated sample of coring, adds liquid nitrogen fast, ground sample, grinding limit, limit adds liquid nitrogen, repeated multiple times, until sample granularity reaches requirement.
In step 1, the core sample carrying out grinding is 2 ~ 3g.
In step 2, the core sample taken is 70 ~ 80mg, and puts into pyrolysis instrument special copple, and puts into liquid nitrogen.
In step 3, start pyrologger, instrument is self-inspection first, at the end of instrument self checking is fast, then is taken out from liquid nitrogen by special copple and puts into crucible position and carry out pyrolysis analysis.
In step 3, pyrolysis instrument analysis condition is: initial temperature 80 DEG C, after retaining 2min, with 25 DEG C/min temperature programme to 300 DEG C, and constant temperature 2min, then with 25 DEG C/min temperature programme to 650 DEG C, constant temperature 1min.
In step 4, identical sample is carried out pyrolysis analysis after normal temperature places 30 days.
The analytical approach of the determination shale pyrolysis Parameter reconstruction coefficient in the present invention, be to choose and newly get core shale samples, it is kept to operate under the condition of liquid nitrogen frozen, reduce the loss of rock gas and lighter hydrocarbons in sample as far as possible, to obtain component relatively complete in shale, and pass through the coefficient of restitution of the pyrolysis parameters of rock determination shale conventional pyrolysis parameter obtained.
Accompanying drawing explanation
Fig. 1 is the process flow diagram determining a specific embodiment of the analytical approach of shale pyrolysis Parameter reconstruction coefficient of the present invention.
Embodiment
For making above and other object of the present invention, feature and advantage can become apparent, cited below particularly go out preferred embodiment, and coordinate institute's accompanying drawings, be described in detail below.
As shown in Figure 1, Fig. 1 is the process flow diagram determining the analytical approach of shale pyrolysis Parameter reconstruction coefficient of the present invention.
In step 101, choose new core-drilling sample and seal freezen protective rapidly.Flow process enters into step 102.
In step 102, open the ventilation of pyrolysis instrument and stablize 2 hours, then carry out school machine, keep holding state.Flow process enters into step 103.
In step 103, liquid nitrogen is poured in copper mortar, and by instrument freezing processing such as pyrolysis instrument special copple, hammer, tweezers, keep it at low-temperature condition.The inner uncontaminated sample 2 ~ 3g of coring puts into the mortar of cooling processing, and add liquid nitrogen fast, ground sample, grinding limit, limit adds liquid nitrogen, repeated multiple times, until sample granularity reaches requirement.Flow process enters into step 104.
In step 104, take sample 70 ~ 80mg fast, put into pyrolysis instrument special copple, and put into liquid nitrogen.In one embodiment, sample 70.25mg is taken fast.Flow process enters into step 105.
In step 105, generalized case, start after sample analysis, instrument is self-inspection first, about 1 ~ 1.5 minute time, and at the end of need treating that instrument self checking is fast, rapider taking-up from liquid nitrogen by crucible is put into crucible position and carried out pyrolysis analysis.Pyrolysis instrument analysis condition is: initial temperature 80 DEG C, after retaining 2min, with 25 DEG C/min temperature programme to 300 DEG C, and constant temperature 2min, then with 25 DEG C/min temperature programme to 650 DEG C, constant temperature 1min.Flow process enters into step 106.
In step 106, same sample normal temperature is placed after 30 days and is carried out pyrolysis analysis, obtains the hydrocarbon content of conventional pyrolysis analysis loss, for calculating coefficient of restitution.Flow process terminates.
According to experimental technique of the present invention, under being made sample be in the environment of low temperature as much as possible by liquid nitrogen in the preservation of core sample, pulverizing, weighing and analyzing and processing process, thus the loss of rock gas and lighter hydrocarbons in minimizing sample, and contrast with conventional pyrolysis analysis, obtain the coefficient of restitution of shale pyrolysis parameter.
Claims (9)
1. determine the analytical approach of shale pyrolysis Parameter reconstruction coefficient, it is characterized in that, this determines that the analytical approach of shale pyrolysis Parameter reconstruction coefficient comprises:
Step 1, grinds core sample, and grinding limit, limit adds liquid nitrogen;
Step 2, takes the sample after grinding, puts into pyrolysis instrument special copple, and special copple is put into liquid nitrogen;
Step 3, takes out special copple and puts into crucible position and adopt pyrolysis instrument to carry out pyrolysis analysis from liquid nitrogen; And
Step 4, carries out pyrolysis analysis by identical sample after normal temperature is placed, and obtains the hydrocarbon content of conventional pyrolysis analysis loss, for calculating coefficient of restitution.
2. the analytical approach determining shale pyrolysis Parameter reconstruction coefficient according to claim 1, is characterized in that, this determines that the analytical approach of shale pyrolysis Parameter reconstruction coefficient also comprises, and before step 1, chooses new core-drilling sample sealing freezen protective; And open pyrolysis instrument stabilizer instrument.
3. the analytical approach determining shale pyrolysis Parameter reconstruction coefficient according to claim 2, is characterized in that, in the step opening pyrolysis instrument stabilizer instrument, opens the ventilation of pyrolysis instrument and stablizes 2 hours, then carry out school machine, keep holding state.
4. the analytical approach determining shale pyrolysis Parameter reconstruction coefficient according to claim 1, it is characterized in that, in step 1, liquid nitrogen is poured in copper mortar, and by pyrolysis instrument special copple, hammer, these instrument freezing processing of tweezers, keep it at low-temperature condition, the mortar of cooling processing put into by the inner uncontaminated sample of coring, adds liquid nitrogen fast, ground sample, grinding limit, limit adds liquid nitrogen, repeated multiple times, until sample granularity reaches requirement.
5. the analytical approach determining shale pyrolysis Parameter reconstruction coefficient according to claim 1, is characterized in that, in step 1, the core sample carrying out grinding is 2 ~ 3g.
6. the analytical approach determining shale pyrolysis Parameter reconstruction coefficient according to claim 1, is characterized in that, in step 2, the core sample taken is 70 ~ 80mg, and puts into pyrolysis instrument special copple, and puts into liquid nitrogen.
7. the analytical approach determining shale pyrolysis Parameter reconstruction coefficient according to claim 1, is characterized in that, in step 3, start pyrologger, instrument is self-inspection first, at the end of instrument self checking is fast, then is taken out from liquid nitrogen by special copple and puts into crucible position and carry out pyrolysis analysis.
8. the analytical approach determining shale pyrolysis Parameter reconstruction coefficient according to claim 1, it is characterized in that, in step 3, pyrolysis instrument analysis condition is: initial temperature 80 DEG C, after retaining 2min, with 25 DEG C/min temperature programme to 300 DEG C, constant temperature 2min, then with 25 DEG C/min temperature programme to 650 DEG C, constant temperature 1min.
9. the analytical approach determining shale pyrolysis Parameter reconstruction coefficient according to claim 1, is characterized in that, in step 4, identical sample is carried out pyrolysis analysis after normal temperature places 30 days.
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| CN112304799A (en) * | 2020-06-24 | 2021-02-02 | 成都理工大学 | Method for quantitatively analyzing organic matters in different occurrence states of shale oil reservoir |
| CN112765765A (en) * | 2020-12-16 | 2021-05-07 | 成都理工大学 | Correction method for pyrolysis result of rock debris of well site oil-based drilling fluid |
| CN112903737A (en) * | 2021-01-21 | 2021-06-04 | 西南石油大学 | Method for evaluating oil content of shale by utilizing pyrolysis before and after extraction |
| CN114199921A (en) * | 2020-08-31 | 2022-03-18 | 中国石油化工股份有限公司 | Method and device for measuring relative content of occurrence state of water in shale |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112304799A (en) * | 2020-06-24 | 2021-02-02 | 成都理工大学 | Method for quantitatively analyzing organic matters in different occurrence states of shale oil reservoir |
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| CN112765765A (en) * | 2020-12-16 | 2021-05-07 | 成都理工大学 | Correction method for pyrolysis result of rock debris of well site oil-based drilling fluid |
| CN112765765B (en) * | 2020-12-16 | 2022-03-01 | 成都理工大学 | Correction method for pyrolysis result of rock debris of well site oil-based drilling fluid |
| CN112903737A (en) * | 2021-01-21 | 2021-06-04 | 西南石油大学 | Method for evaluating oil content of shale by utilizing pyrolysis before and after extraction |
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